Analytical Methods
·
2013
·Vol. 5
·期 22
·6395-6400
·
IF 1.855
Yilin Pan,Ping Xue,Xiang Li,Jianwei Chen,Jin Li
To establish an ultra-high performance liquid chromatography coupled with triple quadrupole mass (HILIC-UPLC-MS/MS) for determination of sixteen nucleosides and nucleobases in Isatidis Radix. Chromatographic separation was carried out on a Acquity UPLC BEH Amide column with gradient elution of acetonitrile (containing 0.1% acetic acid) and water (containing 0.8% acetic acid and 10 mmol L−1 ammonium acetate) at a flow rate of 0.3 mL min−1, the column temperature was set at 35 °C; Waters Xevo™ TQ worked in multiple reaction monitoring mode. Each component were separating in 11 min. All calibration curves were linear (r2 > 0.997) over the tested ranges. The limits of detection of these compounds were 0.02–42.54 ng mL−1. The limits of quantitation of these compounds were 0.05–98.18 ng mL−1. The average recoveries were in the range of 93.81–105.77% with RSD value less than 7.5%. The result showed that almost all of these Isatidis Radix were rich in nucleosides and nucleobases, but their contents were obviously various. The method was simple and fast with high precision, sensitivity and repeatability, which can be used for determination of this type class of nucleosides and nucleobases in other medicinal herbs.
研究领域:
药学
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分析化学
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DOI
高影响因子
Heliyon
·
2023
·
IF 4
Chengcheng Jin,Ting Wang,Tingting Zhao,Wen Jiang,Xiaolan Zhen,Hui Li
Objective To determine the concentrations of nine drugs used in the treatment of cardiovascular diseases in human plasma through QuEChERS pre-treatment combined with ultra-performance liquid chromatography-tandem mass spectrometry. Plasma samples were extracted with 3 mL of acetonitrile, 400 mg of anhydrous magnesium sulfate as a salting agent, and 20 mg of C18 as a sorbent. An Agilent Poroshell 120 EC-C18 column (4.6 × 100 mm, 2.7 μm) was selected and methanol-0.1 % water was used as the mobile phase, and ESI positive ion detection mode was selected. Results: The plasma concentrations of nisoldipine, metoprolol, and prazosin exhibited good linearity within the range of 0.05–4.0 ng/mL (r > 0.99), while atenolol, bisoprolol, propranolol, rosuvastatin, and atorvastatin showed linearity within the range of 0.5–40 ng/mL (r > 0.99). Fluvastatin showed good linearity within the range of 5.0–400 ng/mL. The accuracy of the method ranged from 94.15 to 110.62 %, while the recovery levels were in the range of 85.23 %–115.13 %. The matrix effects were observed between-6.54 % and 12.43 %. The intra-day and inter-day RSD was <15 % for the three concentrations of low, medium, and high. Conclusion The proposed method is rapid, accurate, specific, simple, reproducible, and suitable for the simultaneous measurement of the concentrations of nine drugs used in the treatment of cardiovascular diseases in human plasma.
研究领域:
分析化学
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药理学
·
临床医学
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DOI
高影响因子
MOLECULES
·
2019
·Vol. 24
·期 16
·3016
·
IF 3.06
Ying Xue,Lin-Sen Qing,Li Yong,Xian-Shun Xu,Bin Hu,Ming-Qing Tang,Jing Xie
So far, there is no report on the quality evaluation of lemonade available in the market. In this study, a sample preparation method was developed for the determination of flavonoid glycosides by ultra-performance liquid chromatography–mass spectrometry (UPLC-MS) based on vortex-assisted dispersive liquid-liquid microextraction. First, potential flavonoids in lemonade were scanned and identified by ultra-performance liquid chromatography–time of flight mass spectrometry (UPLC-TOF/MS). Five flavonoid glycosides were identified as eriocitrin, narirutin, hesperidin, rutin, and diosmin according to the molecular formula provided by TOF/MS and subsequent confirmation of the authentic standard. Then, an ultra-performance liquid chromatography–triple quadrupole mass spectrometry (UPLC-QqQ/MS) method was developed to determine these five flavonoid glycosides in lemonade. The results showed that the content of rutin in some lemonade was unreasonably high. We suspected that many illegal manufacturers achieved the goal of low-cost counterfeiting lemonade by adding rutin. This suggested that it was necessary for relevant departments of the state to make stricter regulations on the quality standards of lemonade beverages.Keywords:vortex-assisted dispersive liquid-liquid microextraction;flavonoid glycoside;UPLC-MS;counterfeiting lemonade
研究领域:
分析化学
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食品科学
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药物分析
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Translational and Clinical Pharmacology
·
2021
·
IF 0
Hyeon-Cheol Jeong,Yo-Han Seo,Namyi Gu,Moo Yong Rhee,Kwang-Hee Shin
Candesartan and olmesartan are angiotensin II receptor blockers (ARBs) used for the treatment of hypertension and heart failure. Quantitation methods for candesartan and olmesartan were developed using ultra-high performance liquid chromatography-tandem mass spectrometry following protein precipitation. Candesartan was separated using 5 mM ammonium formate (A) and 100% acetonitrile (B) and olmesartan was separated using 2 mM ammonium formate with 0.1% formic acid (A) and 100% acetonitrile (B). Separation was performed using an isocratic method with a Thermo hypersil GOLD C18 column. Electrospray ionization was used for analyte ionization and detection of candesartan, olmesartan, and the internal standards by multiple reaction monitoring. Developed method showed excellent linearity ( r > 0.99) in the concentration range of 2–500 ng/mL for candesartan and 5–2,500 ng/mL for olmesartan. Accuracies were 86.70–108.8% for candesartan and 87.87–112.6% for olmesartan. These methods were able to successfully measure plasma candesartan or olmesartan concentrations in hypertensive patients. This study can be used for pharmacokinetic studies of candesartan or olmesartan in humans.
研究领域:
药理学
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分析化学
✓ 已验证
DOI
PubMed
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2022
·
IF 4.52
Cuimin He,Weibin Huang,Xianmei Xue,Zhike Liang,Hao Ye,Kunping Li,Xujiang Yuan
Abrus precatorius leaves (APL) are one herb with the function of preventing and treating diabetes and widely used in health care and tea drinking in China. The objective of this study was to investigate the fingerprints, phytochemicals and quality evaluation of flavonoids from APL. Seven flavonoids were isolated and identified by NMR, ESI-MS and UV, with compounds 1–4, 6 from APL for the first time. An UPLC-ESI-Q-TOF/MS method was first established to evaluate the fingerprints. Similarity results showed that the overall quality of APL from different sources was relatively stable, but there were also some content differences, which could be used for regional classification. Total 29 compounds were identified by UPLC-MS/MS. An HPLC method was established to simultaneously determine the contents of seven flavonoids and could be used to identify and distinguish the quality of APL. The content of flavonoids in APL from different sources was 2.31–11.0%. This is the first report on the fingerprints, HPLC method and quality profile of seven flavonoids from APL.
研究领域:
植物化学
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药物分析
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产品关联
DOI
高影响因子
Foods
·
2025
·Vol. 14
·期 10
·1660
·
IF 5.1
Rong Chen,Lan Chen,Mingyue Du,Qiaozhen Guo,Ciping Zhong,Jing Zhang,Xiaoqin Yu
A high-throughput method for the determination of a variety of chemical hazards in poultry muscle and egg samples was established via ultra-performance liquid chromatography–tandem triple quadrupole mass spectrometry (UPLC–QqQ-MS). The sample preparation procedure was developed based on this quick, easy, cheap, effective, rugged, and safe (QuEChERS) method and validated for 280 chemical hazards potentially present in poultry products. The target compounds in poultry samples were extracted with a 1% formic acid–acetonitrile solution (15:85,v/v), and the metal ions in the matrix were chelated by adding ethylenediaminetetraacetic acid disodium salt (Na2EDTA). The supernatant was purified using Enhanced Matrix Removal (EMR) lipid sorbent. Chromatographic gradient separation was performed on an ACQUITY UPLC BEH C18 (2.1 mm × 100 mm, 1.7 μm) column with multiple reaction monitoring (MRM) under both negative- and positive-ion mode. Internal standard calibration or matrix-matched calibration was used for the quantitation. The results showed that good linearity was achieved for each target compound with correlation coefficients (R2) ≥ 0.99. The limits of detection (LODs) ranged from 0.05 to 10 µg/kg, and the acceptable limits of quantification (LOQs) were determined to be 0.1–20 µg/kg for all 280 compounds. Approximately 90% of the target compounds exhibited mean recoveries ranging from 60% to 120%, with relative standard deviations (RSDs) within 16.2%. This method can be used for the high-throughput rapid detection of prohibited drug residues in poultry eggs due to its easy operation and high accuracy. It was applied in real sample detection, and 43 chemicals including metronidazole were found in 211 poultry samples, with a concentration range of 0.11–638 μg/kg.
研究领域:
食品科学
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分析化学
✓ 已验证
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2021
·
IF 3.935
Qinghua Weng,Wei Tan,Ren-yue Yu,Ren-ai Xu,Yu Chen
Pemigatinib is an oral, selective, potent, competitive inhibitor acting on fibroblast growth factor receptor (FGFR)1, FGFR2, and FGFR3, which has obtained accelerated approval in the USA through a test approved by the USA FDA. It is not only significant in the therapy of adult recurrent, unresectable, metastatic or locally advanced cholangiocarcinoma, but also plays an important role in treating adult patients with FGFR2 fusion or other rearrangements. The aim of our research was to establish and verify a reliable and quick ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) assay to determine the level of pemigatinib in rat plasma. The analyte was prepared using a simple and convenient approach with acetonitrile for protein crash, and then separated from the matrix on a Waters Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) in a gradient elution program, where the mobile phase was consisted of acetonitrile and 0.1 % formic acid in water and was set at 0.40 mL/min flow rate. Selective reaction monitoring (SRM) was used to conducted for UPLC-MS/MS dectection with ion transitions at m / z 488.01 → 400.98 for pemigatinib and m / z 447.00 → 361.94 for erdafitinib (Internal standard, IS), respectively. This method had good linearity in a 0.5−1000 ng/mL calibration range for pemigatinib, where the lower limit of quantification (LLOQ) was validated at 0.5 ng/mL. The precision of pemigatinib for intra- and inter-day was less than 13.3 %, and the accuracy was determined to be from −4.8%–11.2%. During the assay in plasma samples, the analyte was found to be stable. Besides, matrix effect and recovery of the analyte and IS were acceptable. The novel optimized UPLC-MS/MS assay was also suitable for determining the concentration level of pemigatinib in a pharmacokinetic study after a single dose of 1.35 mg/kg pemigatinib orally to the rats.
研究领域:
药物分析
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生物化学
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医学研究
✓ 已验证
DOI
高影响因子
JOURNAL OF FOOD SCIENCE
·
2019
·Vol. 84
·期 5
·1138-1144
·
IF 2.081
Jingbo Zhang,Jing Hu,Shuai Wang,Xinping Lin,Huipeng Liang,Shengjie Li,Chenxu Yu,Xiuping Dong,Chaofan Ji
To effectively extract biogenic amines (BAs) from complex food matrices is an important issue. In this study, a stop-and-go-extraction tip (StageTip)-based method for simultaneous enrichment of six BAs including histamine, tyramine, putrescine, cadaverine, tryptamine, and β-phenylethylamine in fish samples was developed and optimized. This StageTip-based BAs extraction method required short extraction time, small sample size, and minimal consumption of organic solvents. In addition, an ultrahigh-performance liquid chromatography coupled with triple quadrupole mass spectrometer was used to identify and quantify BAs without derivatization. Target recovery efficiencies of BAs from spiked fish samples ranged from 84% to 110%. Linear regression models were established to determine BAs in the range of 0.4 to 3.0 mg/L ( R 2 > 0.995). Good repeatability was obtained with relative standard deviation of peak areas (1.17 to 5.61%) and retention time (0.09 to 0.20%). High sensitivity was achieved for the detection of six BAs (0.064 to 1.00 ng/L for the limit of detection, 0.10 to 5 ng/L for the limit of quantification). The proposed method had an obvious advantage in the analysis of BAs in complex food matrices such as fish tissues since it could reflect the subtle distribution of BAs from one fish fillet. Practical Application A StageTip-based BAs enrichment combined with UPLC-MS analysis method was developed and optimized, which was low - cost , environmentally friendly, and with good analytical performances. As such, it has the potential to become a powerful tool for the analysis of BAs in different complex food matrices.
研究领域:
食品科学
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分析化学
✓ 已验证
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2014
·
IF 2.694
Wei-min Zhang,Rui-fang Li,Ming Sun,Da-ming Hu,Jian-fei Qiu,Yun-hao Yan
A rapid, sensitive and selective ultra-performance liquid chromatography tandem mass spectrometry (UPLC–MS/MS) was developed and validated for the determination and pharmacokinetic investigation of avicularin in rat plasma. Sample preparation was accomplished through a simple one-step deproteinization procedure with 0.2 mL of acetonitrile–methanol (9:1, v/v) to a 0.1 mL plasma sample. Plasma samples were separated by UPLC on an Acquity UPLC BEH C18 column using a mobile phase consisting of acetonitrile–0.1% formic acid in water with gradient elution. The total run time was 1.60 min and the elution of avicularin was at 1.20 min. The detection was performed on a triple quadrupole tandem mass spectrometer in the multiple reaction-monitoring (MRM) mode using the respective transitions m / z 434.1 → 301.3 for avicularin and m / z 237.2 → 194.3 for carbamazepine (IS), respectively. The calibration curve was linear over the range of 10–3000 ng/mL with a lower limit of quantitation (LLOQ) of 10 ng/mL. Mean recovery of avicularin in plasma was in the range of 84.2–89.5%. Intra-day and inter-day precision were both <12%. This method was successfully applied in pharmacokinetic study after intravenous administration of 5.0 mg/kg avicularin in rats.
研究领域:
分析化学
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药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
CyTA-Journal of Food
·
2025
·
IF 1.7
Zhou Lu,Zhao Junpeng,Hilary Kwesi Ketemepi
A QuEChERS-UPLC-MS/MS method was developed and validated for simultaneous determination of six pesticides (chlorpyrifos, malathion, carbofuran, thiodicarb, deltamethrin, and lambda-cyhalothrin) in dairy products. Samples (n=50), collected from a supermarket in Chongqing, China, were extracted with 1% acetic acid–acetonitrile, purified using PSA, and quantified by external-standard UPLC-MS/MS. All pesticides showed excellent linearity (0.001–0.50 mg/L, R² > 0.99), with LOQs of 0.002 mg/kg. Average recoveries at four spiking levels (0.002, 0.01, 0.1, 1.0 mg/kg) ranged from 89% to 110% (RSD 0.5–9.5%, n=5). Analysis of real samples revealed residues below China’s MRLs (GB 2763–2021), confirming regulatory compliance. The method meets analytical requirements for dairy matrices and offers a reliable framework adaptable to other international standards.
研究领域:
食品科学
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分析化学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2018
·
IF 0.827
Yang-Fang He,Han-Qing Cai,Wen-Ying Li,Yang Xiu,Wen-Long Liu,Hong-Yue Chi,Hong Shen,Mao-Guang Yang,Jin Pei,Shu-Ying Liu
A quantitative analysis of ginseng chemical ingredients was established using UPLC-MS, in which the concentrations of ginsenosides, oligosaccharides, and amino acids in ginseng were determined. Unlike the C18 column, which showed good performance in the determination of ginsenosides, the NH2 column was used in this method, and it exhibited good separation abilities for three types of compounds, including 6 saponins, 4 oligosaccharides, and 15 amino acids. For each type of compound, a recovery of 88%–111%, with relative standard deviations (RSD) better than 6% (n＝6) were obtained; the limits of quantification (LOQ) for three types of substances were less than 1μg/mL. Furthermore, the method showed strong ability on the discrimination Asia Ginseng and America Ginseng, and was confirmed to be robust, selective, sensitive, rapid and inexpensive.GRAPHICAL
研究领域:
药用植物学
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分析化学
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中药学
✓ 已验证
DOI
高影响因子
MOLECULES
·
2023
·Vol. 28
·期 5
·2022
·
IF 4.6
Ting Zhang,Dingrong Wan,Yuanyuan Li,Sisi Wang,Xiuteng Zhou,Fatemeh Sefidkon,Xinzhou Yang
TheArtemisia argyiLévl. et Van. growing in the surrounding areas of Qichun County in China are called Qiai (QA). Qiai is a crop that can be used both as food and in traditional folk medicine. However, detailed qualitative and quantitative analyses of its compounds remain scarce. The process of identifying chemical structures in complex natural products can be streamlined by combining UPLC-Q-TOF/MS data with the UNIFI information management platform and its embedded Traditional Medicine Library. For the first time, 68 compounds in QA were reported by the method in this study. The method of simultaneous quantification of 14 active components in QA using UPLC-TQ-MS/MS was reported for the first time. Following a screening of the activity of QA 70% methanol total extract and its three fractions (petroleum ether, ethyl acetate, and water), it was discovered that the ethyl acetate fraction enriched with flavonoids such as eupatilin and jaceosidin had the strongest anti-inflammatory activity, while the water fraction enriched with chlorogenic acid derivatives such as 3,5-di-O-caffeoylquinic acid had the strongest antioxidant and antibacterial activity. The results provided the theoretical basis for the use of QA in the food and pharmaceutical industries.Keywords:Artemisia argyiLévl. et Van.;UPLC-MS;quantification;anti-inflammatory;antioxidant
研究领域:
药理学
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分析化学
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传统医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）